# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 207/503 data_kentax_kishikawa_tboeu_98- #------------------------------------------------------------------------------ _audit_creation_date 'Fri May 20 13:45:34 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 327.42 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H25 N O3 ' _chemical_formula_moiety 'C20 H25 N O3 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.665(1) _cell_length_b 9.667(1) _cell_length_c 16.100(1) _cell_angle_alpha 90 _cell_angle_beta 98.060(7) _cell_angle_gamma 90 _cell_volume 1797.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 21.9 _cell_measurement_theta_max 23.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 704.00 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.18 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 0 6 5 -2 1 3 -4 -1 _diffrn_reflns_number 3603 _reflns_number_total 3428 _reflns_number_observed 2013 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 3.75 _diffrn_reflns_av_sigmaI/netI 0.102 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 67.60 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.08028 _diffrn_orient_matrix_UB_12 0.03802 _diffrn_orient_matrix_UB_13 0.00372 _diffrn_orient_matrix_UB_21 -0.02505 _diffrn_orient_matrix_UB_22 0.08528 _diffrn_orient_matrix_UB_23 0.02767 _diffrn_orient_matrix_UB_31 0.02058 _diffrn_orient_matrix_UB_32 -0.04452 _diffrn_orient_matrix_UB_33 0.05618 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 80 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 100 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 12 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags O2 -0.1533(2) 0.1185(2) -0.0139(1) 0.0570(7) Uani d . 1.00 . O3 0.2119(2) 0.3248(2) 0.1560(2) 0.0722(8) Uani d . 1.00 . O4 0.0549(2) -0.0551(3) 0.2606(2) 0.0867(10) Uani d . 1.00 . N2 0.1622(2) 0.1249(3) 0.2193(1) 0.0455(7) Uani d . 1.00 . C1 0.2439(3) 0.1377(3) 0.2948(2) 0.0499(9) Uani d . 1.00 . C2 0.0564(2) 0.1787(3) 0.0881(2) 0.0438(8) Uani d . 1.00 . C3 -0.0064(2) 0.0644(3) 0.1294(2) 0.0463(9) Uani d . 1.00 . C4 0.3541(2) 0.0798(3) 0.3043(2) 0.0458(9) Uani d . 1.00 . C5 0.1516(2) 0.2241(3) 0.1555(2) 0.0474(9) Uani d . 1.00 . C6 0.4211(3) 0.1038(4) 0.3820(2) 0.062(1) Uani d . 1.00 . C7 0.4013(3) -0.0099(3) 0.2380(2) 0.0529(10) Uani d . 1.00 . C8 0.0695(3) 0.0332(4) 0.2105(2) 0.055(1) Uani d . 1.00 . C9 -0.1393(3) 0.2603(4) 0.0159(2) 0.062(1) Uani d . 1.00 . C10 -0.1291(3) 0.1042(4) 0.1425(2) 0.063(1) Uani d . 1.00 . C11 -0.1968(3) 0.1601(4) 0.0626(2) 0.062(1) Uani d . 1.00 . C12 0.3956(3) 0.0636(4) 0.1537(2) 0.072(1) Uani d . 1.00 . C13 -0.0169(3) 0.2999(4) 0.0511(2) 0.061(1) Uani d . 1.00 . C14 0.3325(3) -0.1438(4) 0.2241(3) 0.082(1) Uani d . 1.00 . C15 0.2053(3) 0.2144(5) 0.3577(2) 0.078(1) Uani d . 1.00 . C16 0.3831(3) 0.1797(5) 0.4441(2) 0.083(1) Uani d . 1.00 . C17 0.2752(4) 0.2355(5) 0.4326(2) 0.097(2) Uani d . 1.00 . C19 0.5288(3) -0.0487(5) 0.2646(3) 0.096(2) Uani d . 1.00 . C20 -0.3268(3) 0.1511(6) 0.0584(3) 0.108(2) Uani d . 1.00 . C21 -0.2025(4) 0.3692(4) -0.0406(3) 0.105(2) Uani d . 1.00 . H1 0.4970 0.0661 0.3919 0.0731 Uiso calc . 1.00 . H2 -0.1680 0.0255 0.1601 0.0746 Uiso calc . 1.00 . H3 -0.1246 0.1737 0.1845 0.0746 Uiso calc . 1.00 . H4 0.4418 0.1445 0.1601 0.0844 Uiso calc . 1.00 . H5 0.4230 0.0035 0.1141 0.0844 Uiso calc . 1.00 . H6 0.3174 0.0882 0.1342 0.0844 Uiso calc . 1.00 . H7 -0.0197 0.3658 0.0945 0.0710 Uiso calc . 1.00 . H8 0.0196 0.3403 0.0076 0.0710 Uiso calc . 1.00 . H9 0.2549 -0.1234 0.2020 0.0964 Uiso calc . 1.00 . H10 0.3660 -0.2004 0.1852 0.0964 Uiso calc . 1.00 . H11 0.3352 -0.1914 0.2757 0.0964 Uiso calc . 1.00 . H12 0.1295 0.2542 0.3490 0.0921 Uiso calc . 1.00 . H13 0.4320 0.1928 0.4960 0.0978 Uiso calc . 1.00 . H14 0.2486 0.2890 0.4755 0.1144 Uiso calc . 1.00 . H15 0.5368 -0.0956 0.3166 0.1128 Uiso calc . 1.00 . H16 0.5544 -0.1066 0.2231 0.1128 Uiso calc . 1.00 . H17 0.5745 0.0334 0.2699 0.1128 Uiso calc . 1.00 . H18 -0.3482 0.1794 0.1104 0.1275 Uiso calc . 1.00 . H19 -0.3624 0.2091 0.0148 0.1275 Uiso calc . 1.00 . H20 -0.3507 0.0579 0.0472 0.1275 Uiso calc . 1.00 . H21 -0.1861 0.4581 -0.0166 0.1261 Uiso calc . 1.00 . H22 -0.1755 0.3664 -0.0942 0.1261 Uiso calc . 1.00 . H23 -0.2824 0.3519 -0.0475 0.1261 Uiso calc . 1.00 . H24 0.0927 0.1380 0.0434 0.0525 Uiso calc . 1.00 . H25 -0.0100 -0.0176 0.0943 0.0554 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(2) 0.050(1) 0.061(1) 0.057(1) 0.007(1) -0.005(1) -0.020(1) O(3) 0.056(1) 0.057(2) 0.095(2) -0.017(1) -0.018(1) 0.020(1) O(4) 0.073(2) 0.107(2) 0.077(2) -0.029(2) 0.000(1) 0.039(2) N(2) 0.036(1) 0.054(2) 0.045(1) -0.004(1) 0.000(1) 0.004(1) C(1) 0.045(2) 0.059(2) 0.044(2) -0.005(2) 0.002(1) -0.001(2) C(2) 0.040(2) 0.047(2) 0.044(2) 0.003(1) 0.004(1) 0.000(1) C(3) 0.037(2) 0.052(2) 0.049(2) -0.003(1) 0.003(1) -0.004(2) C(4) 0.045(2) 0.044(2) 0.046(2) -0.007(1) -0.004(1) 0.008(1) C(5) 0.036(2) 0.048(2) 0.056(2) 0.003(1) 0.002(1) 0.003(2) C(6) 0.054(2) 0.070(2) 0.057(2) -0.006(2) -0.010(2) 0.005(2) C(7) 0.049(2) 0.044(2) 0.063(2) 0.003(2) -0.002(2) -0.001(2) C(8) 0.047(2) 0.063(2) 0.056(2) -0.007(2) 0.008(2) 0.007(2) C(9) 0.056(2) 0.054(2) 0.069(2) 0.015(2) -0.018(2) -0.021(2) C(10) 0.042(2) 0.086(3) 0.061(2) -0.006(2) 0.012(2) -0.019(2) C(11) 0.038(2) 0.083(3) 0.064(2) 0.012(2) 0.000(2) -0.029(2) C(12) 0.076(2) 0.067(3) 0.076(3) 0.006(2) 0.029(2) -0.003(2) C(13) 0.058(2) 0.055(2) 0.062(2) 0.006(2) -0.015(2) 0.000(2) C(14) 0.095(3) 0.055(2) 0.093(3) -0.010(2) 0.005(2) -0.007(2) C(15) 0.056(2) 0.111(3) 0.066(2) 0.001(2) 0.008(2) -0.025(2) C(16) 0.076(3) 0.122(4) 0.047(2) -0.021(3) -0.003(2) -0.012(2) C(17) 0.074(3) 0.156(5) 0.062(3) -0.007(3) 0.014(2) -0.041(3) C(19) 0.065(3) 0.091(3) 0.122(4) 0.028(2) -0.017(2) -0.026(3) C(20) 0.041(2) 0.177(5) 0.103(3) 0.017(3) -0.001(2) -0.047(3) C(21) 0.093(3) 0.072(3) 0.130(4) 0.029(2) -0.055(3) -0.018(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00017|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.74(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2013 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0591 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0614 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.911 _refine_ls_shift/esd_max 0.1650 _refine_ls_shift/esd_mean 0.0040 _refine_diff_density_min -0.73 _refine_diff_density_max 1.07 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(2) C(9) 1.453(4) 1_555 1_555 yes O(2) C(11) 1.452(4) 1_555 1_555 yes O(3) C(5) 1.200(3) 1_555 1_555 yes O(4) C(8) 1.203(4) 1_555 1_555 yes N(2) C(1) 1.442(4) 1_555 1_555 yes N(2) C(5) 1.398(4) 1_555 1_555 yes N(2) C(8) 1.390(4) 1_555 1_555 yes C(1) C(4) 1.390(4) 1_555 1_555 yes C(1) C(15) 1.380(4) 1_555 1_555 yes C(2) C(3) 1.529(4) 1_555 1_555 yes C(2) C(5) 1.505(4) 1_555 1_555 yes C(2) C(13) 1.522(4) 1_555 1_555 yes C(2) H(24) 0.968 1_555 1_555 no C(3) C(8) 1.502(4) 1_555 1_555 yes C(3) C(10) 1.525(4) 1_555 1_555 yes C(3) H(25) 0.971 1_555 1_555 no C(4) C(6) 1.398(4) 1_555 1_555 yes C(4) C(7) 1.536(4) 1_555 1_555 yes C(6) C(16) 1.364(5) 1_555 1_555 yes C(6) H(1) 0.950 1_555 1_555 no C(7) C(12) 1.526(5) 1_555 1_555 yes C(7) C(14) 1.522(5) 1_555 1_555 yes C(7) C(19) 1.536(4) 1_555 1_555 yes C(9) C(11) 1.447(5) 1_555 1_555 yes C(9) C(13) 1.510(4) 1_555 1_555 yes C(9) C(21) 1.514(5) 1_555 1_555 yes C(10) C(11) 1.513(5) 1_555 1_555 yes C(10) H(2) 0.949 1_555 1_555 no C(10) H(3) 0.949 1_555 1_555 no C(11) C(20) 1.511(4) 1_555 1_555 yes C(12) H(4) 0.947 1_555 1_555 no C(12) H(5) 0.951 1_555 1_555 no C(12) H(6) 0.952 1_555 1_555 no C(13) H(7) 0.949 1_555 1_555 no C(13) H(8) 0.953 1_555 1_555 no C(14) H(9) 0.946 1_555 1_555 no C(14) H(10) 0.956 1_555 1_555 no C(14) H(11) 0.946 1_555 1_555 no C(15) C(17) 1.373(5) 1_555 1_555 yes C(15) H(12) 0.956 1_555 1_555 no C(16) C(17) 1.358(5) 1_555 1_555 yes C(16) H(13) 0.951 1_555 1_555 no C(17) H(14) 0.950 1_555 1_555 no C(19) H(15) 0.945 1_555 1_555 no C(19) H(16) 0.951 1_555 1_555 no C(19) H(17) 0.953 1_555 1_555 no C(20) H(18) 0.947 1_555 1_555 no C(20) H(19) 0.947 1_555 1_555 no C(20) H(20) 0.952 1_555 1_555 no C(21) H(21) 0.951 1_555 1_555 no C(21) H(22) 0.960 1_555 1_555 no C(21) H(23) 0.939 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(9) O(2) C(11) 59.7(2) 1_555 1_555 1_555 yes C(1) N(2) C(5) 122.7(2) 1_555 1_555 1_555 yes C(1) N(2) C(8) 123.6(3) 1_555 1_555 1_555 yes C(5) N(2) C(8) 112.1(2) 1_555 1_555 1_555 yes N(2) C(1) C(4) 123.4(3) 1_555 1_555 1_555 yes N(2) C(1) C(15) 114.8(3) 1_555 1_555 1_555 yes C(4) C(1) C(15) 121.8(3) 1_555 1_555 1_555 yes C(3) C(2) C(5) 104.3(2) 1_555 1_555 1_555 yes C(3) C(2) C(13) 116.7(2) 1_555 1_555 1_555 yes C(3) C(2) H(24) 108.4(3) 1_555 1_555 1_555 no C(5) C(2) C(13) 112.0(3) 1_555 1_555 1_555 yes C(5) C(2) H(24) 107.4(2) 1_555 1_555 1_555 no C(13) C(2) H(24) 107.6(3) 1_555 1_555 1_555 no C(2) C(3) C(8) 105.2(2) 1_555 1_555 1_555 yes C(2) C(3) C(10) 113.3(3) 1_555 1_555 1_555 yes C(2) C(3) H(25) 108.7(3) 1_555 1_555 1_555 no C(8) C(3) C(10) 112.4(3) 1_555 1_555 1_555 yes C(8) C(3) H(25) 108.3(3) 1_555 1_555 1_555 no C(10) C(3) H(25) 108.8(3) 1_555 1_555 1_555 no C(1) C(4) C(6) 115.1(3) 1_555 1_555 1_555 yes C(1) C(4) C(7) 124.5(3) 1_555 1_555 1_555 yes C(6) C(4) C(7) 120.3(3) 1_555 1_555 1_555 yes O(3) C(5) N(2) 124.1(3) 1_555 1_555 1_555 yes O(3) C(5) C(2) 127.9(3) 1_555 1_555 1_555 yes N(2) C(5) C(2) 108.0(3) 1_555 1_555 1_555 yes C(4) C(6) C(16) 123.1(3) 1_555 1_555 1_555 yes C(4) C(6) H(1) 118.5(4) 1_555 1_555 1_555 no C(16) C(6) H(1) 118.3(3) 1_555 1_555 1_555 no C(4) C(7) C(12) 112.3(3) 1_555 1_555 1_555 yes C(4) C(7) C(14) 110.5(3) 1_555 1_555 1_555 yes C(4) C(7) C(19) 111.8(3) 1_555 1_555 1_555 yes C(12) C(7) C(14) 108.0(3) 1_555 1_555 1_555 yes C(12) C(7) C(19) 106.3(3) 1_555 1_555 1_555 yes C(14) C(7) C(19) 107.7(3) 1_555 1_555 1_555 yes O(4) C(8) N(2) 124.4(3) 1_555 1_555 1_555 yes O(4) C(8) C(3) 127.1(3) 1_555 1_555 1_555 yes N(2) C(8) C(3) 108.4(3) 1_555 1_555 1_555 yes O(2) C(9) C(11) 60.1(2) 1_555 1_555 1_555 yes O(2) C(9) C(13) 114.8(3) 1_555 1_555 1_555 yes O(2) C(9) C(21) 115.8(3) 1_555 1_555 1_555 yes C(11) C(9) C(13) 117.2(3) 1_555 1_555 1_555 yes C(11) C(9) C(21) 123.8(3) 1_555 1_555 1_555 yes C(13) C(9) C(21) 113.8(3) 1_555 1_555 1_555 yes C(3) C(10) C(11) 111.1(3) 1_555 1_555 1_555 yes C(3) C(10) H(2) 109.6(3) 1_555 1_555 1_555 no C(3) C(10) H(3) 108.6(3) 1_555 1_555 1_555 no C(11) C(10) H(2) 109.0(3) 1_555 1_555 1_555 no C(11) C(10) H(3) 108.9(3) 1_555 1_555 1_555 no H(2) C(10) H(3) 109.6(3) 1_555 1_555 1_555 no O(2) C(11) C(9) 60.2(2) 1_555 1_555 1_555 yes O(2) C(11) C(10) 114.8(3) 1_555 1_555 1_555 yes O(2) C(11) C(20) 114.5(3) 1_555 1_555 1_555 yes C(9) C(11) C(10) 117.2(3) 1_555 1_555 1_555 yes C(9) C(11) C(20) 123.4(4) 1_555 1_555 1_555 yes C(10) C(11) C(20) 114.7(3) 1_555 1_555 1_555 yes C(7) C(12) H(4) 109.6(3) 1_555 1_555 1_555 no C(7) C(12) H(5) 109.6(3) 1_555 1_555 1_555 no C(7) C(12) H(6) 109.2(3) 1_555 1_555 1_555 no H(4) C(12) H(5) 109.7(3) 1_555 1_555 1_555 no H(4) C(12) H(6) 109.6(4) 1_555 1_555 1_555 no H(5) C(12) H(6) 109.2(4) 1_555 1_555 1_555 no C(2) C(13) C(9) 113.7(3) 1_555 1_555 1_555 yes C(2) C(13) H(7) 107.7(3) 1_555 1_555 1_555 no C(2) C(13) H(8) 108.6(3) 1_555 1_555 1_555 no C(9) C(13) H(7) 108.6(3) 1_555 1_555 1_555 no C(9) C(13) H(8) 108.9(3) 1_555 1_555 1_555 no H(7) C(13) H(8) 109.3(3) 1_555 1_555 1_555 no C(7) C(14) H(9) 109.6(3) 1_555 1_555 1_555 no C(7) C(14) H(10) 109.2(4) 1_555 1_555 1_555 no C(7) C(14) H(11) 109.5(3) 1_555 1_555 1_555 no H(9) C(14) H(10) 109.2(4) 1_555 1_555 1_555 no H(9) C(14) H(11) 110.1(4) 1_555 1_555 1_555 no H(10) C(14) H(11) 109.3(4) 1_555 1_555 1_555 no C(1) C(15) C(17) 120.6(3) 1_555 1_555 1_555 yes C(1) C(15) H(12) 119.9(3) 1_555 1_555 1_555 no C(17) C(15) H(12) 119.4(4) 1_555 1_555 1_555 no C(6) C(16) C(17) 120.3(3) 1_555 1_555 1_555 yes C(6) C(16) H(13) 119.9(4) 1_555 1_555 1_555 no C(17) C(16) H(13) 119.8(4) 1_555 1_555 1_555 no C(15) C(17) C(16) 119.0(4) 1_555 1_555 1_555 yes C(15) C(17) H(14) 120.4(4) 1_555 1_555 1_555 no C(16) C(17) H(14) 120.5(4) 1_555 1_555 1_555 no C(7) C(19) H(15) 109.6(4) 1_555 1_555 1_555 no C(7) C(19) H(16) 109.5(3) 1_555 1_555 1_555 no C(7) C(19) H(17) 109.2(3) 1_555 1_555 1_555 no H(15) C(19) H(16) 109.8(4) 1_555 1_555 1_555 no H(15) C(19) H(17) 109.6(4) 1_555 1_555 1_555 no H(16) C(19) H(17) 109.1(5) 1_555 1_555 1_555 no C(11) C(20) H(18) 109.4(3) 1_555 1_555 1_555 no C(11) C(20) H(19) 109.4(4) 1_555 1_555 1_555 no C(11) C(20) H(20) 109.2(4) 1_555 1_555 1_555 no H(18) C(20) H(19) 109.9(4) 1_555 1_555 1_555 no H(18) C(20) H(20) 109.5(5) 1_555 1_555 1_555 no H(19) C(20) H(20) 109.5(4) 1_555 1_555 1_555 no C(9) C(21) H(21) 109.3(3) 1_555 1_555 1_555 no C(9) C(21) H(22) 109.2(4) 1_555 1_555 1_555 no C(9) C(21) H(23) 109.8(4) 1_555 1_555 1_555 no H(21) C(21) H(22) 108.6(5) 1_555 1_555 1_555 no H(21) C(21) H(23) 110.3(4) 1_555 1_555 1_555 no H(22) C(21) H(23) 109.6(4) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(2) C(3) 3.321(4) 1_555 3_555 ? O(2) C(2) 3.368(4) 1_555 3_555 ? O(3) C(19) 3.345(4) 1_555 2_655 ? O(3) C(21) 3.487(5) 1_555 3_565 ? O(4) C(13) 3.425(4) 1_555 2_545 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_kentax_kishikawa_tboeu_98- #------------------------------------------------------------------------------ _audit_creation_date 'Fri May 20 13:45:34 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 327.42 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H25 N O3 ' _chemical_formula_moiety 'C20 H25 N O3 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.665(1) _cell_length_b 9.667(1) _cell_length_c 16.100(1) _cell_angle_alpha 90 _cell_angle_beta 98.060(7) _cell_angle_gamma 90 _cell_volume 1797.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 21.9 _cell_measurement_theta_max 23.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 704.00 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.18 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 0 6 5 -2 1 3 -4 -1 _diffrn_reflns_number 3603 _reflns_number_total 3428 _reflns_number_observed 2013 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 3.75 _diffrn_reflns_av_sigmaI/netI 0.102 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 67.60 _diffrn_reflns_reduction_process 'Lp correctio